Separating and collecting particles of one liquid suspended in another liquid.



. F. G'. GOTTRELL & J. B. SPEED. v SEPARATING AND COLLECTING PARTICLES OF ONE LIQUID SUSPENDED IN ANOTHER LIQUID. I

APPLICATION FILED MAY 20, 1909. RENEWED OCT. 12, 1911).

Patented Mar. 21, 1911.

UNITED STATES PATENT OFFICE.

FREDERICK GARDNER COTTRELL AND JAMES I BUCKNER SPEED, OF BERKELEY, CALI FOBNIA, ASSIGNORS, BY MESNE ASSIGNMENTS, TO PETROLEUM RECTIFYING COM- IPANY, OF SAN FRANCISCO, CALIFORNIA, A CORPORATION OF CALIFORNIA.

SEIARATIN'G AND COLLECTING PARTICLES OF ONE LIQUID S USPENDED IN ANOTHER LIQUID.

Specification of Letters Patent.

Patented Mar. 21, 1911.

Application filed May 20, 1909, Serial No. 497,167? Renewed October 12, 1910. Serial No. 586,794.

' rating mechanical mixtures of liquids such as emulsionsof water in oil, and to methods or processes of such separatlon.

In order to present our invention 1n a concrete and easily understandable form, we

wi1l,-at the outset, describe it as applied to. the separation and removal of water particles from crude petroleum, but it is to be understoodthat' we do not limit our claims to this particular case.

Much of the crude petroleum as it comes from the wells contains drops of water,

varying in size from thoseeasily visible to the naked eye to 'a minuteness lying at the extreme range of vision of the most powerful microscope. In some cases this water settles out upon standing, and this may be accelerated by heating the mass, and-by treating it in various forms of centrifugal separators. Thefirstof these methods is very generally employed and, the centrifugal treatment has received a great deal of study and has to-day a certain limited applicability, but, at present. there still remains a I k large class of 011s that cannot be economically freed fromzwater without distillation.

These are largely oils inwhich the water is in very small globules often less than one thousandth of an inch in diameter and behaving as if surrounded with a membrane-,;; IQSISiIIlg coalescence of the dro.ps. In manyg; cases, however, distillation is prohlbltlvely' expensive, and even where it is desired eventually to distil the'oil it is of great technicaladvantage to be able to first, temove'sus pended water, as its presence tends to. produce explosive boiling and running over of the still contents, on the one hand, and. on

theqother hand, to ioulingof the still bottoms; eventually leading to badheat con-. ductlvity carbonization,' and, finally, de-

struction-of the materials of construction of the still itself.

Many natural pe'troleums, as taken from the wells, contain from- 7 to 50% ofwater in form of small drops (2'. e. emulsions) and after being allowed to stand for months still hold a great proportion of the water in-suspension. We have found that when the same emulsions are subjected to the acetion of high potential electric charges in the manner described below, they are rapidly deemulsified, the water settling to the bottomof the vessel, and collecting into large masses which can be readily withdrawn, 'leaving'the oil dry. As much of the mechanically suspendedsolids in the oil are carried in or on these water globules, the process also eliminates a great proportion of these, and in fact Where it 'is desired to remove suspended solids from an oil con taming no water globules this may be accomplished by churning the, oil up with water-to such an emulsion, and then applying the treatment as described below, the solids being largely carried down by the water droplets in their coalescence, although the same treatmentjapnlied to the dryv oil containing the dry solids in suspension 'without the water, occasions little, if any, removal of said solids. The mechanism of the phenomenon may be followed under the microscope, if. a thin layer of emulsified der these conditions the water drops or M globules in the oil immediately commence to arrange themselves in chains extending 1 out from each electrode toward the other,

strongly suggesting filaments of yeast cells: as'seen in a fermenting liquor. Rapidly following the formation of the chains comes a coalescence of the adjacent globules in each chain, and as. the chain" accumulates newparticles, chiefly at the free ends, the drops nearest the electrodes vabecfome the largest, successive members of the chain d1m1n1sh1ng' fairly regularly in size as'the free end .is ap the water soon The process of coalescence of reaches a point where the latter rapidly separates out in irregular masses or films on the electrodes and supporting slide.

The above phenomenon may be obtained with either direct or alternating current source of electricity, but for'technical purposes, at. least, the latterhas decided advantages. In case direct current is used there is superimposed upon the above described phenomenon a second, via, the streaming bodily of the liquid from one electrode to the other, due to cat-aphoresis along the more intense force lines, which tends to disrupt the chains of globules and prevent their formation and coalescence. between the phenomenon as produced by' a] ternating and direct current must be clearly recognized in distinguishing our process from the various applications which-have heretofore been made of the phenomenon of cataphoresisor electric endosmosc which depend upon causing particles suspended in liquids to migrate from one electrode of constant polarity toward another of opposite polarity, and are, direct current systems.

preached.

In the process here described and claimed these phenomena are merely incidental, and, sometimes, a positive disadvantage, as we rely instead-upon the coalescing action possessed also by the alternating current, where it is observed stripped of the direct migrations found in the case of the direct current. The process must, further, be distinguished from those among which fall; for example, the various applications of electric current to the purification of water whichdepend on relmoval of dissolved electrolytes by ionic m1- gration; (2) acceleration of sedimentation of suspended matterby roduction of chemical compounds at the e ectrodes by electrochemical reactions; and killing of organisms by electric curr nt. In the present process we are "dealing with a typicalnonconductor, oil, in which are suspended globtiles of a substance which compared with the oil has a very appreciable conductivity viz. water often carrying considerable safyline matter in solution. .These globules are thereby subjected to electrostatic forces de-. the relative potentials "a nd which may be readily removed from the body of the oil by well known processes such as settling. I I a p y In addition t'o"its greater actual effectiveness, the alternating current presents the further important technical advantages, that it is far easier with it to obtain highvoh ta es which are most advantageous for ban-- ante-g large masses of .materialon account iofthe greater--; .dist ance between the elec- This distinction high. potential therefore, limited to trodes which they permit, and, also, the danger of electrolytic corrosion of, the apparatus is nating, rather than of the direct current.

Having thus outlined certain of the basic principles upon which ratus by the use of which these prinei les eliminated by the use of the alterthe present .method "is founded, we will next describe an appaniay be carried out in practice, and t en with the concrete illustration as a basis, prokreed to discuss some of the more important details of the process.

Referring to the accompanyingdrawing- Figure 1- is ageneral view of a complete set of apparatus, diagrammatically illustrated, by means of which the process may be carried out. Fig. 2 is a plan of the electrically treating vessel.

A is a vessel, containing the oil undergoing the electrical treatment and itself serves as one of the. electrodes, being connected to the ground and. also to one of the terminals of the step-up transformer T. The other 'high potential terminal of the transformer is connected to the electrode C represented in the figure as an .inner shell concentric with the, wall of the vessel A and supported thereon by the insulators I, I I, and the spider '8. low potential terminals of the transformer are connected through the ammeter M and regulating rheostat R with the electric service mains, as, for example, lighting circuit. ture to be treated is received through thepipe P, and is heated to any desired temperature for the purpose of decreasing its viscosity, by the injection of live steam through the' pipe Q.- The other inlet U serves to introduce either oil alrea dy treated, or sludge or even water,

The mixture enters the top of the treating vessel through the tangentially directed jets p, 11 19 17 thus insuring a thorough 1111K mg and uniform composition at the top of an incandescent The oil and water mix- The 103 as described below.

thetreating vessel, as'well as occasioning a steady motion of the surface of the liquid the lines of force of the electric field, thus lessening the tendency to. electrical leakage, and break-down inthe surface layers. The material thus supplied to the top ofthe vessel flows uniformily down through the annularspace around the inner electrode where the electrical treatmentchiefly occurs, and is finally carried-out of. the bottom of the treating vessel A through the pipe D which is of largeenough diameter to insure a quiet flow free from churning that might tend to reemulsifythe separating liquids. The pipe D discharges into the settling tank E, preferably its lower portiomwherc the final separation of the .oil and water is accoinplished, the latter being drawn off tovresidual sludge, through geth er vvith any in the funnel shaped top at right angles to of its intake endwithin the tank, as indivessel A.

cated inthe' figure by the flexible joint g,

and the adjusting cord 9 passing over the pulleys 9 ,9 As for any any given rate of how, the level in the tank E also determines the level inthe vessel A, this adjustment serves to control the level of material in The chief reason shaped top of the vessel A hes in our discovery that it is essential for the proper working of the method not to allow the-essentially active surfaces ofthe electrodes (by which term is to be understood those portions which are in sufficient proximity to the electrode of opposite polarity to be really efiicient in produc: ing coalescenceof the intervening suspended particles) to emerge from the liquid undergoing treatment into the air, or even come too close to the surface of contactbetween air and liquid in close proximit' another; for when this" happens t ere is-a decided tendency for the part ally agglomerated water to collect in these surface layers and cause short circuiting of the electrodes.

Care must, therefore, be taken to have the active portion of the electrodes deeply im.-

mersed in the liquid under treatment, as ..is the case in the illustration. 'On account of the funnel shaped top of the vessel, the onl portion of the suspended electrode C which no difiicult further advantage of the above described arrangement lies in the fact that the upper surface of the material in the treating vessel is continually renewed and stirred by "the inflow ofinntreated oil which is a better inleakage.

sulator than'that which is in the incipient stages of chain building and coalescence in the deeper parts of the vessel, thus still further reducing the tendency to surface an important detail as it prevents the danger of short circuitsfrom an accumulation of water-rich masses between the electrodes procedugre which deserves special mention is the heating of theoil by injection of, steam directly i ginto it., "This method of heating ,although one off the most eflicient and con venient possible, is inadvisable in most cases ther than'ths'pre'sent, because of'the finely V innl'sified conditionin which the condensed so con- I for adopting the funnel to one The downward direct-ion of flow between the active electrode surfaces is also reh'larg ed droplets is water is apt to be left in the oil. In the present process this feature is so specifically provided for by the subsequent electrical treatment as to present no drawback, and

hence the combination with the rest of the process of. this means of rendering the oil mdre; fluid and adaptable to the electrical and settling treatment becomes an essential part of our improvements in themethod of treatment.

Still another important feature which our investigation has brought out is the.

. any given character of oil and water mixture and arrangement of electrodes, the ammeter M will show an essentially constant current with only slight irregular variation, or, at most, on y occasional momentary variations of any appreciable magnitude, but if the rheostat resistance be gradually increased, a

condition. will finally be reached where the ammeter reading rapidly increases to several times its or1g1nal value, thus greatly increasing the power consumption, while, at the same time, the potential difference between the electrodes falls, and the effectiveness of comes into these surface layers is at so much greater distance from the wall of the vessel than its deeper active portion, as-to. occasion Z In this same connection, a. Z

A small resistance in series until the primary is advantageol'ls as protection against destructive momentary overloads. We believe theexplanation of this phenomenon to lie in the disruptive force s either electrostatic or thermal which the high potential can exert on these chains of water particles when closed,

or just as they are closing between the electrodes. If the potential falls too low then these forces are overcome by the attractive forces between the articles and permanent electrolytically con noting chains are established between the electrpdes thereby reducing the potential difference of the latter still more and wasting a large part of the supplied energy in useless-"heat of electrolytic conduction.

In many cases a single treatment-as above outlined is all that is required but when necessary the process may be repeated in a separatevessel either with or without intermediate settling and applied to either or both the oil drawn off at G in the first treatmentor any oil and sludge carriedofl" at F with the water. Or this latter material may be returned through the pipe U and thoroughly commingled with the inflowing oil .through the jets.

Another modification of the process which may prove especially useful in case of very high water content of the original oil, con sists in returning a considerable portion of the purified oil from G to U and thus diluting up the oil to be treated. This also facilitates the handling of such oil supplies as may vary considerably from time to time in their water content inasmuch as by regulation of the amount of the dry oil thus added, the conditions within the treating tank may be maintained constant.

The apparatus herein shown, forms no part of the present application and is not herein claimed, as it constitutes a part of the subject matter of a contemporaneous applicatiom serial Number 497,168 filed May 20, 1909.

It is of course to be understood'that the a particular arrangement of electrodes. and

general mode of construction of apparatus above illustrated and described are merely illustrative and that we do notlimitourselves to this or ,any other specific form of apparatus for carrying out the method here described and claimed.

Having thus described our invention what we claim as new and-desire to secure by Letters Patent is: a

. 1. The improvement in the art of separating and collecting particles of one liquid suspended in another liquid which latter is essentially a non-conductor of electricity,

consisting inhringing the material to be electrodes.

treated between electrodes connected to a source of electricity ofsufiicient voltage to produce coalescence of the suspended particles in such wise as to cause the rapid separation of the two liquids throughout the body of the mixture and, at the same time, prevent the coalescing globules from forming complete chains short circuiting. the

2. The improvement in the art of separating and collecting particles of one liquid suspended in another liquid which latter is essentially a non-conductor of electricity,

consisting in bringing the; material to. be treatedbetween electrodes connected to a source of alternating current of sutlicient voltage to produce coalescence of the suspended particles in sucln wise asto cause the rapid separation of the two liquids and, at the same time, prevent the coalescing globules from forming completechains short circuiting the electrodes.

3. The improvement in the art of separating and collecting particles of one liquid suspended in another liquid which latter is essentially a non-conductor of electricity, conslstmg in causing the mater1al to be treated to flow between electrodes whose essentially active surfaces are immersed below the surface layers of said material, and are-connected to a source of electricityof sufiicient voltage to produce coalescence'of the suspended particles in such wise as to cause the rapid separation of the two liquids throughout the body of the mixture and, at the same time, prevent the coalescing globules from forming complete chains short circuiting the electrodes.

4. The improvement in the art of separatingand collecting particles of a liquid suspended in' another liquid relatively lighter and which is essentally a non-conductor of electricity, which consists in causing the material to be treated to flow downward between electrodes whose essentially active surfaces are immersed'below the sur face layers of said material, and are connected to a source of electricity of sufficient voltage to produce coalescence of the suspended particles in such wise as to-cause the rapid separation of the two liquids throughout the body of the mixture and, at the same time, prevent the coalescing globules from forming complete chains short circuiting the electrodes.

5. The improvement in the art of separating and collecting particles of a liquid suspended in another liquid relatively lighter and which is essentially a non-conductor of electricity, which consists in causing the material to be treated to enter the electrical treating vessel in the form of streams impinging upon the upper surface of the liquid contents of the vessel in such manneras to cause a-stirring of said surface and thorough mixmg of said inflowing ma; terial, and thence to flow downward between electrodes whose essentially active' surfaces are immersed below the surface layers of said material, and are connected to a source of electricity of sufficient voltage toproduce coalescence of the suspended particles in such wise as to cause the rapid separation of the two liquids and, atthe same'time, prevent the coalescing globules from'forming complete chains short circuit;

ing the electrodes. 7

6. The improvement in the art of separating and collecting particles of a liquid suspended in another liquid relatively lighter and which is essentially a non-conductor of.electricity,- which consists in first decreasing the viscosity of the mixture by the direct inj eetioninto it of live steam, and

then bringing the resulting material between electrodes connected to a source of electricity of suflicient voltage to produce coalescence of the suspended particles in such wiseas' to causethe rapid separation of the two liquids and, at the same time, prevent the coalescing globules from forming complete chains short circuiting the electrodes.

7. The improvement in the art of separating and collecting particles of one liquid suspended in another liquid which latter is essentially a non-conductor of electricity, which consists in first passing the material to be treated between charged electrodes substantially as described, and then causing said material to flow quietly and Without churning action into a settling reservoir from the top of which the lighter, and from the bottom of which the heavier of the two liquids are, respectively, withdrawn.

8. The improvement in the art of separating and collecting particles of one liquid suspended in another liquid which latter is essentially a non-conductor of electricity,

consisting in, first, comminglin terial to be treated with material rom which the mathe suspended particles have already been removed and, then, bringing the mixtures, thus formed, between electrodes connected to a source of electricity of sufficient voltage to produce coalescence of the suspended particles in such Wise as to cause the rapid separation of the two liquids and, at the same time, prevent the coalescing globules from forming complete chains short circuiting the electrodes. I

. In testimony whereof we have signed our names to this specification in the presence of two subscribing Witnesses.

FREDERICK GARDNER COTTRELL.

JAMES BUGKNER SPEED, Witnesses:

' WM. F. BOOTH,

D. B. RICHARDS. 

